EP1292539B1 - Sulfate de baryum micronise - Google Patents

Sulfate de baryum micronise Download PDF

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Publication number
EP1292539B1
EP1292539B1 EP01934015A EP01934015A EP1292539B1 EP 1292539 B1 EP1292539 B1 EP 1292539B1 EP 01934015 A EP01934015 A EP 01934015A EP 01934015 A EP01934015 A EP 01934015A EP 1292539 B1 EP1292539 B1 EP 1292539B1
Authority
EP
European Patent Office
Prior art keywords
process according
sulphate
barium
solution
concentration
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP01934015A
Other languages
German (de)
English (en)
Other versions
EP1292539A1 (fr
Inventor
Ferdinand Hardinghaus
Tanja Engels
Jai-Won Park
Karl Köhler
Hans Gabel
Jörg GLAS
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Solvay Infra Bad Hoenningen GmbH
Original Assignee
Solvay Barium Strontium GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Solvay Barium Strontium GmbH filed Critical Solvay Barium Strontium GmbH
Publication of EP1292539A1 publication Critical patent/EP1292539A1/fr
Application granted granted Critical
Publication of EP1292539B1 publication Critical patent/EP1292539B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/23—Sulfur; Selenium; Tellurium; Compounds thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/46—Sulfates
    • C01F11/462—Sulfates of Sr or Ba
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/027—Barium sulfates
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area

Definitions

  • the invention relates to a particulate Barium sulfate, its production and use.
  • Barium sulfate can be used as a pigment in papermaking, for example.
  • other applications such as an additive for cosmetics such as skin creams and sunscreen creams, as an additive (filler) in paints, adhesives or rubber articles, require the Ba-SO 4 to be extremely fine.
  • the object of the present invention is an effective Process for the production of a finely divided, particulate micronized barium sulfate to indicate which as an additive for cosmetics or as a filler for paints, adhesives or rubber articles can be used. This task is by the inventive method and what is available Product solved.
  • the process according to the invention for the production of particulate barium sulfate provides that a barium salt solution is combined with a sulfate salt solution in a continuously operating mixing reactor, in which the shear, shear and frictional forces of intermeshing tools with a high relative speed according to the rotor-stator principle act the reaction mixture formed, and the barium sulfate formed is separated from the reaction mixture after passing through the reactor and dried, with the proviso that the concentration of barium salt or sulfate corresponds to at least 80%, preferably at least 90% of the maximum possible concentration.
  • the shear, shear and friction forces in the reactor cause the barium sulfate to be formed in an extremely finely divided form.
  • barium hydroxide is also understood as a salt that can be used.
  • the most technically expedient is BaCl 2 solution.
  • the concentration of Ba salt in the solution advantageously corresponds to at least 95% of the maximum possible concentration. In the case of BaCl 2 , this is approximately at least 0.9 mol / l at 60 ° C.
  • sulfate solution encompasses solutions of any aqueous sulfate salts.
  • sulfuric acid is also regarded as a "sulfate solution”.
  • concentration is preferably at least 95% of the maximum possible concentration up to the saturation limit.
  • An aqueous alkali sulfate solution is preferably used.
  • Alkali is preferably sodium.
  • concentration of Na 2 SO 4 is preferably (at 40 ° C.) at or above 0.5 mol / l up to the saturation concentration.
  • micronized barium sulfate is obtained, in which at least 90% of the particles have a primary grain diameter smaller have as 0.1 ⁇ m, preferably at least 95%, in particular at least 99%, especially 100%.
  • the rotor speed is preferably 2,000 to 8,000 revolutions / sec.
  • the dwell time the reaction mixture in the mixing and homogenizing device is preferably in the millisecond range.
  • the grain size was assessed using microscopic images.
  • the BaSO 4 separated off after passing through the reactor can be washed with water one or more times.
  • the advantage of using barium hydroxide / sulfuric acid is that no foreign salt (e.g. NaCl) is formed.
  • the precipitation of barium sulfate is useful in one Temperature in the range from 0 to 100 °, preferably from 20 ° C. up to 50 ° C.
  • no agent is added the crystallization or the surface properties affected.
  • Another object of the invention is the particulate Barium sulfate, which by the inventive method is available in which at least 90% of the primary grain particles a diameter in the range of less than 0.1 ⁇ m, and which is free of precipitation aids.
  • the BaSO 4 obtainable in this way according to the invention can be used for all purposes for which BaSO 4 is generally used. It is particularly good as an additive for cosmetics (it also has a reflective, scattering and refractive effect). For this purpose, it is used in appropriate formulations, for example as a cream.
  • the formulations obtained, the z. B. used as a sunscreen are superior to formulations with TiO 2 as a pigment (UV light stabilizer), since no visible residues remain on the skin after being absorbed. If desired, you can incorporate a sunscreen; This means that the sun protection factor can be adjusted individually depending on its quantity, and the cream or formulation can be used as a sunscreen.
  • the BaSO 4 obtainable according to the invention is also distinguished by a marked improvement in the feeling on the skin.
  • a network or Dispersant added. This can occur during the precipitation, after precipitation or during and after precipitation.
  • the wetting or dispersing agent should lead to the fact that small crystals form that agglomerate as little as possible.
  • the wetting or dispersing agents also influence the Surface properties of barium sulfate, it is namely a coated product.
  • Dispersants can be used or wetting agents for aqueous and non-aqueous Systems. You choose the dispersant so that it in Is compatible in terms of application. Hydrophilic Dispersants are used advantageously if this property is desirable, provided the base materials of the Adhesive, color or cosmetics also hydrophilic are. Otherwise, hydrophobic dispersants are chosen accordingly out.
  • the particles coated according to the invention with adjustable surface properties is one tailor-made adaptation to the desired application technology Properties possible.
  • Dispersants that can be used well are (shorter-chain) polyacrylates, usually in the form of the sodium salt; polyether like polyglycol ether; Ether sulfonates such as lauryl ether sulfonate in the form of the sodium salt; Esters of phthalic acid and their derivatives; Esters of polyglycerol; Amines such as triethanolamine; and esters of fatty acids such as stearic acid esters are useful.
  • the amount of dispersant is flexible.
  • a very finely divided product with a very high surface area is achieved with a content of up to 3% by weight of the dispersant, based on the total weight of the dry product.
  • the content in the finished product is advantageously 1 to 3% by weight (dry matter).
  • Obtained barium sulfate is also the subject of the invention.
  • the resultant particle size below 100, preferably below 50 nm redispersible coated barium sulfate is particularly suitable good as an additive (filler) for adhesives (for example Reactive, hot melt and dispersion adhesives), for rubber articles, for paints (e.g. topcoats, basecoats or Primer) and for cosmetics (e.g. for UV absorption, or for Skincare or Lipcare products).
  • adhesives for example Reactive, hot melt and dispersion adhesives
  • paints e.g. topcoats, basecoats or Primer
  • cosmetics e.g. for UV absorption, or for Skincare or Lipcare products.
  • the coated barium sulfate is inert, transparent and conveys advantageous reological properties to the application matrix. It is in solvents or the base materials redispersible for adhesives, paints, cosmetic or rubber articles. By choosing the appropriate dispersant it is also compatible with the materials used. The tailor-made coating adjustment is therefore possible.
  • a mixing reactor with a rotor was used Had a speed of 6,650 rpm; the rotor practiced accordingly Shear, thrust and frictional forces on the mixture of Reactants.
  • This cream containing BaSO 4 was also creamy and absorbed into the skin without residue. There was also no formation of agglomerates.
  • the sun protection factor can be set individually become.
  • the cream is then also used as a sunscreen usable.
  • Example 1 was repeated. However, sodium polyacrylate (product Dispex N40, Ciba) was added to the Na 2 SO 4 solution. The amount was such that the finished dried product contained 3% by weight of the dispersant.
  • sodium polyacrylate product Dispex N40, Ciba
  • the coated barium sulfate obtained had a specific surface area of 48 m 2 / g (BET method) and an average particle diameter of 30 nm (wide-angle X-ray diffractometry, modified Warren-Averbach method) in the primary grain (measurement without redispersion).
  • This product is an additive for paints, rubber articles and adhesives particularly well suited because of the dispersant acts as a binding agent.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Birds (AREA)
  • Dermatology (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Epidemiology (AREA)
  • Geology (AREA)
  • Cosmetics (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Compounds Of Unknown Constitution (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Medicinal Preparation (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Claims (12)

  1. Procédé pour l'obtention de sulfate de baryum particulaire, dans lequel au moins 90% des particules ont un diamètre de noyau primaire inférieur à 0,1 µm, dans lequel on met une solution de sel de baryum en contact avec une solution de sel de sulfate alcalin avec formation d'un mélange réactionnel dans un réacteur de mélange fonctionnant en continu, dans lequel les forces cisaillement, de poussée et de frottement des outils venant en prise avec une vitesse relative élevée agissent sur le mélange réactionnel formé, et, après passage dans le réacteur, on sépare du mélange réactionnel le sulfate de baryum formé et on le fait sécher à la condition que la concentration en sel de baryum ou en sulfate corresponde à au moins 80%, de préférence au moins 90% de la concentration maximale possible.
  2. Procédé selon la revendication 1, caractérisé en ce qu'on lave une plusieurs fois à l'eau le sulfate de baryum séparé avant le séchage.
  3. Procédé selon la revendication 1, caractérisé en ce qu'on effectue la précipitation du sulfate de baryum à une température dans la plage de 0°C à 100°C, de préférence 20°C à 50°C.
  4. Procédé selon la revendication 1, caractérisé en ce que la vitesse de rotation du rotor est de 2.000 à 8.000 tr/mn.
  5. Procédé selon la revendication 1, caractérisé en ce que le temps de séjour du mélange réactionnel dans le réacteur de mélange est de l'ordre de la milliseconde.
  6. Procédé selon la revendication 1, caractérisé en ce qu'on utilise des solutions aqueuses.
  7. Procédé selon la revendication 1, caractérisé en ce qu'on utilise une solution de BaCl2.
  8. Procédé selon la revendication 7, caractérisé en ce que la concentration en BaCl2 est d'au moins 0,9 mole/l.
  9. Procédé selon la revendication 1, caractérisé en ce que, comme solution de sulfate alcalin, on utilise une solution de sulfate de sodium.
  10. Procédé selon la revendication 1, caractérisé en ce que la solution de sulfate de sodium a une concentration en Na2SO4 d'au moins 0,9 mole/l.
  11. Procédé selon la revendication 1, caractérisé en ce que, pendant et/ou après la précipitation, on utilise un agent mouillant ou un agent dispersant.
  12. BaSO4 revêtu particulaire, dans lequel au moins 95%, de préférence au moins 99%, en particulier 100% des particules présentent un diamètre de noyau primaire inférieur ou égale à 0,1 µm, après le procédé selon la revendication 11.
EP01934015A 2000-05-31 2001-05-26 Sulfate de baryum micronise Expired - Lifetime EP1292539B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10026791A DE10026791A1 (de) 2000-05-31 2000-05-31 Mikronisiertes Bariumsulfat
DE10026791 2000-05-31
PCT/EP2001/006031 WO2001092157A1 (fr) 2000-05-31 2001-05-26 Sulfate de baryum micronise

Publications (2)

Publication Number Publication Date
EP1292539A1 EP1292539A1 (fr) 2003-03-19
EP1292539B1 true EP1292539B1 (fr) 2004-05-19

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EP01934015A Expired - Lifetime EP1292539B1 (fr) 2000-05-31 2001-05-26 Sulfate de baryum micronise

Country Status (14)

Country Link
US (2) US20030124048A1 (fr)
EP (1) EP1292539B1 (fr)
JP (1) JP2003535010A (fr)
CN (1) CN1207210C (fr)
AT (1) ATE267145T1 (fr)
AU (1) AU2001260332A1 (fr)
BR (1) BR0111233A (fr)
DE (2) DE10026791A1 (fr)
DK (1) DK1292539T3 (fr)
ES (1) ES2221900T3 (fr)
HK (1) HK1053823A1 (fr)
PT (1) PT1292539E (fr)
RU (1) RU2283813C2 (fr)
WO (1) WO2001092157A1 (fr)

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DE3703377C2 (de) * 1987-02-05 1994-05-19 Metallgesellschaft Ag Verfahren zur Herstellung von ultrafeinem Bariumsulfat durch Fällung
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ATE267145T1 (de) 2004-06-15
BR0111233A (pt) 2003-06-10
RU2283813C2 (ru) 2006-09-20
US20030124048A1 (en) 2003-07-03
WO2001092157A1 (fr) 2001-12-06
CN1431971A (zh) 2003-07-23
RU2002133214A (ru) 2004-03-27
CN1207210C (zh) 2005-06-22
JP2003535010A (ja) 2003-11-25
US7001582B2 (en) 2006-02-21
DE10026791A1 (de) 2001-12-06
EP1292539A1 (fr) 2003-03-19
AU2001260332A1 (en) 2001-12-11
ES2221900T3 (es) 2005-01-16
HK1053823A1 (en) 2003-11-07
US20040197262A1 (en) 2004-10-07
DK1292539T3 (da) 2004-06-28
PT1292539E (pt) 2004-09-30
DE50102337D1 (de) 2004-06-24

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